WO1989000081A1 - Adsorbent - Google Patents

Adsorbent Download PDF

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Publication number
WO1989000081A1
WO1989000081A1 PCT/JP1987/000467 JP8700467W WO8900081A1 WO 1989000081 A1 WO1989000081 A1 WO 1989000081A1 JP 8700467 W JP8700467 W JP 8700467W WO 8900081 A1 WO8900081 A1 WO 8900081A1
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WO
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Prior art keywords
adsorbent
uranium
metal
oxygen
containing atmosphere
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Application number
PCT/JP1987/000467
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French (fr)
Japanese (ja)
Inventor
Yoshio Tsunoda
Original Assignee
Yoshio Tsunoda
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Publication of WO1989000081A1 publication Critical patent/WO1989000081A1/en

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
    • C22B60/02—Obtaining thorium, uranium, or other actinides
    • C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
    • C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
    • C22B60/0252—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries
    • C22B60/0265—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries extraction by solid resins
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention relates to a novel adsorbent. More specifically, the present invention relates to an adsorbent effective for recovering a useful substance present at a relatively low concentration in a large amount of a solution from the solution, and particularly, the adsorbent according to the present invention is present in a trace amount in seawater. It is useful for recovery of heavy metals such as uranium. Background art
  • activated carbon, ion-exchange resin, zeite light, activated alumina, silicate, and the like have been generally used to recover heavy metals present at a relatively low concentration in a solution.
  • various studies have been conducted on adsorbents used for recovering uranium, especially for recovering uranium from seawater.
  • Such adsorbents include metal oxides and hydroxides as inorganic ones.
  • Substances, sulfides, and pherocyanic compounds are known, and among them, many studies have been made on the hydroxides of titanium (see, for example, Senoo et al. 154 (1 984), ibid. 4, p. 218 (1 984), etc.].
  • the present inventor has conducted intensive studies to develop an adsorbent having a high adsorptivity for heavy metals such as uranium, and as a result, a product obtained by subjecting a mixture of a metal oxide and a metal sulfur compound to a heat treatment is: Surprisingly, it was found that heavy metals such as uranium exhibit much higher adsorption capacity than titanic acid, which has been known as one of the adsorbents with high adsorption capacity. The present invention has been reached.
  • At least one selected from the first group consisting of a metal oxide and a metal compound which generates a metal oxide by heating at a high temperature in an oxygen-containing atmosphere is mixed with at least one kind selected from the second group consisting of a metal sulfur compound and a metal compound part or all of which forms a metal sulfur compound by high-temperature heating in an oxygen-containing atmosphere, Subject to high temperature heating in oxygenated atmosphere there is provided an adsorbent characterized by comprising the product obtained thereby.
  • the first group of metal oxides and metal compounds include ⁇ , ⁇ , ⁇ , ⁇ , AA, IVB, VA, WB. And ⁇ in the periodic table.
  • Oxides and compounds of the elements belonging to the groups of the following groups may be mentioned.
  • Examples of the metal compound which partially or entirely generates a metal oxide by heating at a high temperature in an oxygen-containing atmosphere, for example, in air include: Hydroxide, carbonate, oxalate and the like. It should be noted that the use of the above metal compound (for example, oxalate) as an adsorbent for the obtained adsorbent rather than using the oxide of the above element in advance as the first group substance It has been found that the performance is generally better.
  • Examples of the second group of metal sulfur compounds and metal compounds include sulfides and sulfur compounds of elements belonging to each of the above-mentioned groups in the periodic table, and include those in an oxygen-containing atmosphere, for example, in the air.
  • Examples of the metal compound that partially or wholly generates a metal sulfur compound by heating and heating include, for example, sulfate. .
  • a mixture of at least one first component selected from the first group and at least one second component selected from the second group is mixed in an oxygen-containing atmosphere, for example, in air.
  • the heating temperature may be a temperature at which the mixture becomes a burning state, and is not particularly limited, but is generally about 700 to about 800 ° C.
  • the heating time is not particularly critical, but is generally about 5 to 15 minutes. It is.
  • the weight ratio of the first component to the second component is generally 0.5 to 3, preferably 1 to 2, in weight ratio.
  • the resulting product is generally in powder form and is very easy to handle.
  • the product thus obtained can be used as it is as the adsorbent of the present invention, but can be used in combination with other adsorbents.
  • the adsorption operation can be performed as follows.
  • the first method is a method in which a powdery adsorbent is put into seawater and sufficiently stirred, and then the sorbent and the seawater are separated by a sedimentation method or an excess method. It is not practical because it requires a large device for separation and takes a long time for the operation, and there are many other difficulties.
  • a powdery adsorbent is granulated with an appropriate granulating agent to form a granular adsorbent, which is filled into a column or the like, and seawater is passed through the column in a different manner.
  • Uranium is adsorbed, and then uranium is desorbed and recovered from the adsorbent.
  • the third method is a method utilizing the fact that the adsorbent of the present invention is generated by heating at a high temperature. That is, the raw material of the adsorbent according to the present invention is mixed with a substance that can be formed by heating, for example, clay, and the mixture is appropriately shaped.
  • This is a method in which a heat treatment is performed to form a molded article having an arbitrary shape containing an adsorbent, and this is subjected to, for example, the second method. This is a very industrially advantageous method.
  • the desorbed uranium can be desorbed by a conventional method using a mineral acid such as hydrochloric acid.
  • the novel adsorbent according to the present invention has an extremely high adsorptivity for heavy metals such as uranium, its production method is simple, and its handling is easy. If it is used for the recovery of uranium, its extremely high adsorption capacity will enable industrial uranium collection. Further, as shown in Examples, the adsorption of heavy metals to the adsorbent of the present invention can be achieved only by bringing the adsorbent of the present invention into contact with the solution containing the heavy metal to be recovered for a short period of time. It is extremely advantageous in industry.
  • the adsorbent of the present invention is prepared at a high temperature, there is a feature that the adsorbent retains the adsorption ability even at a high temperature. This is advantageously applied, for example, to the purification of a liquid at a high temperature.
  • aqueous solution having a uranium equilibrium concentration of 1 g / ⁇ was prepared by adding a 1 wt. Aqueous solution of peranyl sodium carbonate to distilled water to prepare a test solution. This test solution (80 m ⁇ ) was placed in Erlenmeyer-I-Frasco (200 ⁇ J8), and the above-mentioned adsorbent (1 g) was added thereto, followed by stirring well at room temperature for 1 minute. Next, this was separated, and uranium in the door liquor was quantified to determine the amount of adsorption. As a result, the amount of uranium adsorbed per gram of the adsorbent was 58 mg.
  • an aqueous solution having a uranium concentration of 10 ⁇ g / ⁇ was prepared in the same manner as described above and used as a test solution.
  • This test solution 20J2 was placed in a 30 ⁇ container, and the above-mentioned binding agent (50 mg) was added thereto, followed by stirring at room temperature for 1 minute. Next, this was separated, and the amount of silane in the obtained solution was quantified to determine the amount of adsorption.
  • the amount of uranium adsorbed per gram of adsorbent was 1.2 mg.
  • the amount of adsorbent prepared from 1 part by weight of lead sulfide, 1 part by weight of lead oxalate, and 2 parts by weight of oxalic acid is the amount of adsorbent 1 when the uranium equilibrium concentration is 1 g / ⁇ . It was 59 mg per g.
  • the amount of permeated uranium in artificial seawater with an equilibrium uranium concentration of 3 ⁇ & / & was 2000 / ig per gram of adsorbent.

Abstract

An adsorbent is prepared by mixing at least one member selected from a first group consisting of metal oxides and metal compounds capable of partly or wholly forming metal oxides when heated in an oxygen-containing atmosphere with at least one member selected from a second group consisting of metal sulfides and metal compounds capable of partly or wholly forming metal sulfides when heated in an oxygen-containing atmosphere, and heating the mixture in an oxygen-containing atmosphere. This adsorbent has a remarkably high ability of adsorbing heavy metals such as uranium. This adsorbent, which is easy to handle and can be produced with ease, enables recovery of uranium from sea water on an industrial scale because of its remarkably high adsorbing ability.

Description

明細書 吸着剤 技術分野  Description Adsorbent Technical Field
本発明は新規な吸着剤に関する。 更に詳細には、 大量 の溶液から該溶液中に比較的低濃度で存在する有用物質 を回収するのに効果的な吸着剤に関し、 特に、 本発明に よる吸着剤は海水中に微量に存在する ウラン等の重金属 の回収に有用なものである。 背景技術  The present invention relates to a novel adsorbent. More specifically, the present invention relates to an adsorbent effective for recovering a useful substance present at a relatively low concentration in a large amount of a solution from the solution, and particularly, the adsorbent according to the present invention is present in a trace amount in seawater. It is useful for recovery of heavy metals such as uranium. Background art
従来、 溶液中に比較的低濃度で存在する重金属の回収 には、 一般に、 活性炭、 イオン交換樹脂、 ゼ才ライ ト、 活性アルミナ、 シ リケ一 ト等が用い られている。 又、 ゥ ランの回収、 特に海水からのウランの回収に用いられる 吸着剤についても種々の研究がなされており、 それらの 吸着剤は、 無機系のものと しては、 金属酸化物、 水酸化 物、 硫化物、 フ エ ロ シア ン化合物などが知られており、 中でもチタ ンの水酸化物については数多く の研究がなさ れている 〔例えば、 妹尾他 「日本海水学会誌」 3 , P . 154 ( 1 984 ) , 同誌 4， P . 218 ( 1 984 )など〕。 又、 有機系 のものと しては、 高分子吸着剤が種々研究されており、 例えば、 アルソ ン酸基を有する合成樹脂、 アミ ドォキシ ム樹脂、 その他種々のキ レー ト樹脂が知られている〔例 えば、 K . Suga saka et al . , Sep . Sci . Techno l . , 16 , 9 71 ( 198 1 )〕。 Conventionally, activated carbon, ion-exchange resin, zeite light, activated alumina, silicate, and the like have been generally used to recover heavy metals present at a relatively low concentration in a solution. In addition, various studies have been conducted on adsorbents used for recovering uranium, especially for recovering uranium from seawater. Such adsorbents include metal oxides and hydroxides as inorganic ones. Substances, sulfides, and pherocyanic compounds are known, and among them, many studies have been made on the hydroxides of titanium (see, for example, Senoo et al. 154 (1 984), ibid. 4, p. 218 (1 984), etc.]. Various organic adsorbents have been studied as organic ones, and for example, synthetic resins having arsonic acid groups, amidoxime resins, and various other chelating resins are known. [Example For example, K. Suga saka et al., Sep. Sci. Technol., 16, 971 (1981)].
しかし、 これら公知の吸着剤の多く はその吸着能が低 く、 実用に供するには困難な状態である。 発明の開示  However, many of these known adsorbents have low adsorbability and are in a state that is difficult to put to practical use. Disclosure of the invention
上記のよう に、 いまだ実用に酎える吸着剤が提案され ていない現状において、 吸着能の格段に優れた吸着剤が 得られ ば、 重金属類を必要とする工業、 特にウラン源 に問題のある原子力産業にとって極めて有益なものとな る。  As mentioned above, in the current situation where adsorbents that can be used practically have not been proposed, if an adsorbent with remarkably excellent adsorption capacity can be obtained, nuclear industry that requires heavy metals, especially problems with uranium sources It will be very useful for industry.
本発明者は、 ウランなどの重金属類に対して高い吸着 能を有する吸着剤を開発すべく鋭意研究の結果、 金属酸 化物及び金属硫黄化合物の混合物を灼熱処理して得られ る生成物が、 驚くべきこ と に、 ウランなどの重金属に対 して、 これまで吸着能の高い吸着剤の一つと して知られ ているチタン酸に較べて、 遥かに高い吸着能を示すこと をを知見し、 本発明に到達したものである。  The present inventor has conducted intensive studies to develop an adsorbent having a high adsorptivity for heavy metals such as uranium, and as a result, a product obtained by subjecting a mixture of a metal oxide and a metal sulfur compound to a heat treatment is: Surprisingly, it was found that heavy metals such as uranium exhibit much higher adsorption capacity than titanic acid, which has been known as one of the adsorbents with high adsorption capacity. The present invention has been reached.
即ち、 本発明によれば、 金属酸化物及び含酸素雰西気 中での高温加熱によってその一部又は全部が金属酸化物 を生成する金属化合物よ りなる第 1群から選ばれた少な く とも 1種と、 金属硫黄化合物及び含酸素雰囲気中での 高温加熱によってその一部又は全部が金属硫黄化合物を 生成する金属化合物よ りなる第 2群から選ばれた少なく とも 1種と を混合し、 含酸素雰囲気中で高温加熱に付す こ と によっ て得られる生成物よ り なる こ と を特徴とする 吸着剤が提供される。 That is, according to the present invention, at least one selected from the first group consisting of a metal oxide and a metal compound which generates a metal oxide by heating at a high temperature in an oxygen-containing atmosphere. One kind is mixed with at least one kind selected from the second group consisting of a metal sulfur compound and a metal compound part or all of which forms a metal sulfur compound by high-temperature heating in an oxygen-containing atmosphere, Subject to high temperature heating in oxygenated atmosphere There is provided an adsorbent characterized by comprising the product obtained thereby.
本発明において、 第 1群の金属酸化物及び金属化合物 と しては、 周期律表の Ι Β 、 Π Α、 Π Β 、 ΠΙ Α、 ΠΙ Β 、 IV A、 IV B 、 V A、 W B . 及び观の各族に属する元素の 酸化物及び化合物が挙げられ、 含酸素雰囲気中、 例えば 空気中、 での高温加熱によってその一部又は全部が金属 酸化物を生成する金属化合物と しては、 例えば、 水酸化 物、 炭酸塩、 シユ ウ酸塩などが挙げられる。 なお、 第 1 群物質と して、 上記元素の酸化物をあ らかじめ調製して 用いるよ リ も上記金属化合物（例えばシユ ウ酸塩など）を 用いた方が、 得られる吸着剤の吸着能は一般によ り良好 である こ と が知見されている。  In the present invention, the first group of metal oxides and metal compounds include Ι, Π, 、, Α, AA, IVB, VA, WB. And の in the periodic table. Oxides and compounds of the elements belonging to the groups of the following groups may be mentioned. Examples of the metal compound which partially or entirely generates a metal oxide by heating at a high temperature in an oxygen-containing atmosphere, for example, in air, include: Hydroxide, carbonate, oxalate and the like. It should be noted that the use of the above metal compound (for example, oxalate) as an adsorbent for the obtained adsorbent rather than using the oxide of the above element in advance as the first group substance It has been found that the performance is generally better.
第 2群の金属硫黄化合物及び金属化合物と しては、 周 期律表の上記の各族に属する元素の硫化物及び硫黄化合 物が挙げられ、 含酸素雰囲気中、 例えば空気中、 での高 温加熱によってその一部又は全部が金属硫黄化合物を生 成する金属化合物と しては、 例えば、 硫酸塩などが挙げ りれる。.  Examples of the second group of metal sulfur compounds and metal compounds include sulfides and sulfur compounds of elements belonging to each of the above-mentioned groups in the periodic table, and include those in an oxygen-containing atmosphere, for example, in the air. Examples of the metal compound that partially or wholly generates a metal sulfur compound by heating and heating include, for example, sulfate. .
上記の第 1群よ り選ばれた少な く とも 1種の第 1成分 と第 2群よ リ選ばれた少な く とも 1種の第 2成分を混合 し、 含酸素雰囲気中、 例えば空気中にて高温加熱に付す。 加熱温度は、 該混合物が灼熱状態になる温度であればよ く 、 特に限定はないが一般に約 700〜約 800 °Cである。 加 熱時間も特に臨界的ではないが、 一般に、 5 〜 1 5分位 である。 A mixture of at least one first component selected from the first group and at least one second component selected from the second group is mixed in an oxygen-containing atmosphere, for example, in air. To high temperature heating. The heating temperature may be a temperature at which the mixture becomes a burning state, and is not particularly limited, but is generally about 700 to about 800 ° C. The heating time is not particularly critical, but is generally about 5 to 15 minutes. It is.
第 1成分の第 2成分に対する量比は重量比で一般に 0 . 5〜 3、 好ま し くは 1 〜 2 が用いられる。  The weight ratio of the first component to the second component is generally 0.5 to 3, preferably 1 to 2, in weight ratio.
高温加熱処理後、 放冷する。 得られる生成物は一般に 粉状であ り、 取り扱いは極めて容易である。  After high temperature heat treatment, allow to cool. The resulting product is generally in powder form and is very easy to handle.
このよう にして得られる生成物はそのま 本発明の吸 着剤と して用いること ができるが、 他の吸着剤との併用 も可能である。 本発明による吸着剤を用いて、 例えば 海水中のウランを回収しょう とする場合、 吸着操作は次 のよ う に して行なう こ と ができる。  The product thus obtained can be used as it is as the adsorbent of the present invention, but can be used in combination with other adsorbents. When, for example, uranium in seawater is to be recovered using the adsorbent according to the present invention, the adsorption operation can be performed as follows.
その第一の方法は、 海水中に粉末状の吸着剤を投入し、 十分攪拌してから咴着剤と海水と を沈降法または 過等 で分離する方法であるが、 この方法は、 攪拌及び分離の ために大装置を必要とする上に該操作のために長時間を 要したリ 、 その他困難なこ とが多く 、 余り実用的ではな い  The first method is a method in which a powdery adsorbent is put into seawater and sufficiently stirred, and then the sorbent and the seawater are separated by a sedimentation method or an excess method. It is not practical because it requires a large device for separation and takes a long time for the operation, and there are many other difficulties.
その第二の方法は、 粉末状の吸着剤を適当な造粒剤で 造粒して、 粒状吸着剤となし、 これをカラム等に充填し、 その中に海水を違鐃的に通過せしめてウランを吸着させ、 次に吸着剤からウランを脱着して回収する方法である。 この方法は工業的に有利である。  In the second method, a powdery adsorbent is granulated with an appropriate granulating agent to form a granular adsorbent, which is filled into a column or the like, and seawater is passed through the column in a different manner. Uranium is adsorbed, and then uranium is desorbed and recovered from the adsorbent. This method is industrially advantageous.
その第三の方法は、 本発明の吸着剤が高温加熱によつ て生成されることを利用する方法である。 即ち、 本発明 による吸着剤の原料と、 加熱によって成形されう る物質、 例えば粘土等とを混合し、 適当に賦形したのち、 これを 加熱処理して吸着剤を含む任意の形状の成形物とな し、 これをたとえば第二の方法に供する方法である。 これは 工業的に非常に有利な方法である。 The third method is a method utilizing the fact that the adsorbent of the present invention is generated by heating at a high temperature. That is, the raw material of the adsorbent according to the present invention is mixed with a substance that can be formed by heating, for example, clay, and the mixture is appropriately shaped. This is a method in which a heat treatment is performed to form a molded article having an arbitrary shape containing an adsorbent, and this is subjected to, for example, the second method. This is a very industrially advantageous method.
吸着されたウランを脱着する方法はいろいろあるが、 例えば、 塩酸のごとき鉱酸を用いて常法によ り脱着する こと ができる。 産業上の利用可能性  There are various methods for desorbing the adsorbed uranium. For example, the desorbed uranium can be desorbed by a conventional method using a mineral acid such as hydrochloric acid. Industrial applicability
上記のよ う に、 本発明による新規な吸着剤は、 ウラン などの重金属に対して極めて高い吸着能を有しており、 その製造方法も簡単で、 取り扱いも容易であ り、 特に海 水からのウ ランの回収に用いればその極めて高い吸着能 によって工業的なウラン採集が実現できるものである。 また、 本発明の吸着剤への重金属の吸着は、 実施例で示 した如く 、 本発明の吸着剤と回収すべき重金属を含有す る溶液と を短時間接触させるだけで達成されるので、 ェ 業的に極めて有利である。 さ らに、 本発明の吸着剤は高 温下で調製されるため、 高温でも吸着能を保持している 特徵がある。 この こ とは、 例えば高温下における液の精 製等に有利に適用される。 発明を実施するための最良の形態  As described above, the novel adsorbent according to the present invention has an extremely high adsorptivity for heavy metals such as uranium, its production method is simple, and its handling is easy. If it is used for the recovery of uranium, its extremely high adsorption capacity will enable industrial uranium collection. Further, as shown in Examples, the adsorption of heavy metals to the adsorbent of the present invention can be achieved only by bringing the adsorbent of the present invention into contact with the solution containing the heavy metal to be recovered for a short period of time. It is extremely advantageous in industry. Furthermore, since the adsorbent of the present invention is prepared at a high temperature, there is a feature that the adsorbent retains the adsorption ability even at a high temperature. This is advantageously applied, for example, to the purification of a liquid at a high temperature. BEST MODE FOR CARRYING OUT THE INVENTION
実施例 1  Example 1
硫化鉛粉末 1重量部とシユウ酸第一鍚粉末 2重量部と をよ く混合し、 ルツボ内にて約 7 0 0 °Cで 1 0分間加熱 した後、 冷却した。 得られた生成物は、 薄灰褐色の粉末 であった。 これを吸着剤と してウランの吸着実験を行な つた。 1 part by weight of lead sulfide powder and 2 parts by weight of oxalic acid primary powder are mixed well and heated in a crucible at about 700 ° C for 10 minutes After that, it was cooled. The resulting product was a light grey-brown powder. Uranium adsorption experiments were performed using this as an adsorbent.
蒸溜水に炭酸ゥラニルナ 卜リ ウムの 1重量 水溶液を加 えて、 ウラン平衡濃度 1 g / β の水溶液を調製し、 試験液 と した。 この試験液 80 m β を、 200 πι J8 のエルレンマイヤ 一フ ラスコ に入れ、 これに上記の吸着剤 l gを加え、 室温 で 1分間よ く攪拌した。 次にこれを沪別して、 ί戸液中の ウランを定量し、 吸着量を求めた。 その結果、 吸着剤 l g 当 りのウラン吸着量は 58m gであった。  An aqueous solution having a uranium equilibrium concentration of 1 g / β was prepared by adding a 1 wt. Aqueous solution of peranyl sodium carbonate to distilled water to prepare a test solution. This test solution (80 mβ) was placed in Erlenmeyer-I-Frasco (200 πι J8), and the above-mentioned adsorbent (1 g) was added thereto, followed by stirring well at room temperature for 1 minute. Next, this was separated, and uranium in the door liquor was quantified to determine the amount of adsorption. As a result, the amount of uranium adsorbed per gram of the adsorbent was 58 mg.
次に、 上記と同様の方法でウラン濃度 10 μ g/ β の水溶 液を調製して試験液と した。 この試験液 20 J2 を 30 β の容 器に入れ、 これに上記扱着剤 50 m gを加え、 室温で 1分間 よ く攪拌した。 次にこれを护別し、 得られた沪液中のゥ ランを定量し、 吸着量を求めた。 吸着剤 l g当りのウラン 吸着量は 1 . 2mgであった。  Next, an aqueous solution having a uranium concentration of 10 μg / β was prepared in the same manner as described above and used as a test solution. This test solution 20J2 was placed in a 30β container, and the above-mentioned binding agent (50 mg) was added thereto, followed by stirring at room temperature for 1 minute. Next, this was separated, and the amount of silane in the obtained solution was quantified to determine the amount of adsorption. The amount of uranium adsorbed per gram of adsorbent was 1.2 mg.
比較例 1  Comparative Example 1
公知の吸着剤であるチタ ン酸を用いて、 上記と同様の ウラン吸着実験を行なったところ、 ウラ ン平衡濃度が 1 g/ β の場合、 吸着剤 1 g当りのウラン吸着量は 4 mgで あつだ  A similar uranium adsorption experiment was performed using titanic acid, a known adsorbent, and when the uranium equilibrium concentration was 1 g / β, the amount of uranium adsorbed per gram of adsorbent was 4 mg. Hot
- 実施例 2〜 1 5  -Examples 2 to 15
表 1 に示した粉末状の第 1成分及び粉末状の第 2成分 と をよ く混合し、 実施例 1 と同様にして各吸着剤を得た。 得られた各吸着剤を実施例 1 と同様のウランの吸着実験 を行ない、 吸着量を調べた。 その結果を表 1 に示す 表 1 c The powdery first component and the powdery second component shown in Table 1 were mixed well, and each adsorbent was obtained in the same manner as in Example 1. Uranium adsorption experiment using the obtained adsorbents in the same manner as in Example 1. And the amount of adsorption was determined. The results are shown in Table 1 Table 1c
D 宝倫お ί [ 原料 ^量 * D Bao-Lun ί [Raw material ^ Quantity *
No. » 1 β¾ 77 (吸着剤 1 g No. »1 β¾ 77 (Adsorbent 1 g
、盧 部) 、皇 ClP =1 リ vj g J, Robe), Emperor ClP = 1 li vj g J
9 シユ ウ酸 硫化鉛（1) 9 Lead sulphate (1)
笛一 {^)\  Fueichi (^) \
m ま Λ 、 ^ノ  m
、 ζ、ノ ユ ノ ffift ¾ - ffi t  , Ζ, no yu no ffift ¾-ffi t
亜鉛（2) (1)  Zinc (2) (1)
4 シユ ウ酸 硫化鉛（1) 3 0 マグネシ  4 Lead oxalate (1) 3 0 Magnesium
ゥ ム (2)  ゥ mu (2)
5 、ノ、ノ ュ τ Pノ Sef  5, no, no τ P no Sef
¾¾ H¾ ¾! 、丄ノ 1 8 第一鍚（2)  ¾¾ H¾ ¾!, 丄 ノ 1 8 1st 鍚 (2)
6 シユ ウ酸 硫化鉛（1) 2 0 第一鉄（2)  6 Lead oxalate (1) 2 0 Ferrous iron (2)
、ジ レ 1  , Gilet 1
ニ ゥ ム  Nimu
才 キシ ク ロ  Talent
ラ イ ド（0.4)  Light (0.4)
7 シユ ウ酸 硫化鉛（1) 1 0 第一鉄（2)  7 Lead oxalate (1) 1 0 Ferrous iron (2)
酸化ラ ン  Lan oxide
タ ン（0.4) 8 シユウ酸 硫化鉛（1) 1 6 第一鉄（2) Tan (0.4) 8 Lead oxalate (1) 1 6 Ferrous iron (2)
酸化  Oxidation
セ リ ウム  Cerium
(0.4)  (0.4)
9 スピネル型 疏化鉛（1) 2 9 酸化ァルミ  9 Spinel lead phosphide (1) 2 9 Alumi oxide
ニゥ厶 ·  Nimes ·
マグネシ ゥム（  Magnesium (
10 2)  10 2)
1 0 シユウ酸 硫化鉛（1) 7  1 0 Lead sulphate (1) 7
マンガン（2)  Manganese (2)
1 1 シユウ酸 琉化鉛（1) 9  1 1 Lead oxalic acid (1) 9
ニッケル（2)  Nickel (2)
15 1 2 シユ ウ酸 硫化亜鉛 8 第一鉄（2) (1)  15 1 2 Oxalic acid Zinc sulfide 8 Ferrous iron (2) (1)
1 3 シユウ酸 硫化鉄（1) 1 0  1 3 Oxalic acid Iron sulfide (1) 1 0
1 酸化 1 oxidation
20 ジルコ 硫化鉛（1) 1 7  20 Zircon Lead sulfide (1) 1 7
ニゥム（1.3) 1 5 シユ ウ酸 Nimu (1.3) 1 5 Oxalic acid
硫酸鉛（1) 4 2  Lead sulfate (1) 4 2
シユ ウ酸  Oxalic acid
鉛（2)  Lead (2)
(註） *平衡濃度がウランと して 1 g/ β の場合の吸着量 実施例 16  (Note) * Adsorption amount when the equilibrium concentration is 1 g / β as uranium Example 16
硫化鉛 1重量部、 シユ ウ酸鉛 1重量部、 シユ ウ酸第一鍚 2重量部よ り調製した吸着剤の吸着量は、 ウ ラ ン平衡濃 度 1 g/ β の場合、 吸着剤 1 g当 り 59 mgであっ た。  The amount of adsorbent prepared from 1 part by weight of lead sulfide, 1 part by weight of lead oxalate, and 2 parts by weight of oxalic acid is the amount of adsorbent 1 when the uranium equilibrium concentration is 1 g / β. It was 59 mg per g.
またウラン平衡濃度が 3 μ &/ & の人工海水における ゥ ラン Ρ及着量は、 吸着剤 1 g当 り 2000 /i gであっ た。  The amount of permeated uranium in artificial seawater with an equilibrium uranium concentration of 3 µ & / & was 2000 / ig per gram of adsorbent.

Claims

請求の範囲 The scope of the claims
金属酸化物及び含酸素雰囲気中での高温加熱によって その一部又は全部が金属酸化物を生成する金属化合物よ リなる第 1群から選ばれた少なく とも 1種と、 金属硫黄 化合物及び含酸素雰囲気中での高温加熱によってその一 部又は全部が金属硫黄化合物を生成する金属化合物よ り なる第 2群から選ばれた少なく とも 1種とを混合し、 含 酸素雰囲気中で高温加熱に付すことによって得られる生 成物よ りなることを特徵とする吸着剤。  At least one selected from the first group consisting of a metal oxide and a metal compound which partially or entirely forms a metal oxide when heated at a high temperature in an oxygen-containing atmosphere, and a metal sulfur compound and an oxygen-containing atmosphere At least one selected from the second group consisting of a metal compound, a part or all of which forms a metal sulfur compound by high-temperature heating in an atmosphere, and subjecting the mixture to high-temperature heating in an oxygen-containing atmosphere. An adsorbent characterized by comprising the product obtained.
PCT/JP1987/000467 1985-12-27 1987-07-03 Adsorbent WO1989000081A1 (en)

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* Cited by examiner, † Cited by third party
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US8124213B2 (en) * 2008-05-30 2012-02-28 Corning Incorporated Flow-through sorbent comprising a metal sulfide

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4941868B1 (en) * 1970-05-01 1974-11-12
JPS5049181A (en) * 1973-08-31 1975-05-01
JPS5013727B1 (en) * 1969-06-06 1975-05-22
JPS5276284A (en) * 1975-12-18 1977-06-27 Inst Francais Du Petrole Method of removing mercury exist in gases or liquids
JPS5456089A (en) * 1977-10-12 1979-05-04 Kyowa Kagaku Kougiyou Kk Desulfurizing agent

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5013727B1 (en) * 1969-06-06 1975-05-22
JPS4941868B1 (en) * 1970-05-01 1974-11-12
JPS5049181A (en) * 1973-08-31 1975-05-01
JPS5276284A (en) * 1975-12-18 1977-06-27 Inst Francais Du Petrole Method of removing mercury exist in gases or liquids
JPS5456089A (en) * 1977-10-12 1979-05-04 Kyowa Kagaku Kougiyou Kk Desulfurizing agent

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